Granular article containing cellulose ether and wax



Patented May 13, 1941 UNITED STATE S A N-T Y No Drawing. Application June 19 39, summer-mus This invention relates to a granular article consisting of a lower alkyl ether of cellulose and a wax, and to a method whereby the said article having certain desired characteristics may be produced. I

It is among the objects of the invention to provide a free-flowing article consisting offa uniform mixture of a wax and a cellulose lower'alkyl ether which'will mix easily with resins and plasticizers to form homogeneous light-colored melts.

A further object is to make agranular article of uniform composition consisting of a cellulose etherandawax. s

These objects are attained according to the invention by mixing an aqueous dispersion of water. For example, "an alcoholic solutionof ethyl cellulose may be poured into water and the mixture stirred to precipitate the ethyl cellulose particles I in the i swelled, absorptive condition.

, Another way in'which the suspension of the cellulose ether may be prepared in preferred rpm is. to" stir or beat the cellulose "ether'in an aqueous medium the presence or a water miscible solvent and swelling agent'iforthe cellulose ether, such as methanoK-ethanoI, or acetone in concentrationtoo 10w to dissolve-theether but' high molten wax with finely divided water-wet cellulose lower alkyl ether. Examples of methods of carrying out this process are: p

EXAMPLE 1 Solid wax is added to hot water (at a temperature, for example, of between 90 and 95 C.) and, when it is melted, it is dispersed throughoutthe water by vigorous agitation. An oil-in-water type emulsion of a cellulose lower alkyl ether solution is slowly added to the agitated molten wax dispersion. The solvent contained in the'emulsion begins to evaporate on addition to the hot wax dispersion, and to hasten this process the mixture is heated, for example, by blowing steam through it. The cellulose ether precipitatescand immediately absorbs wax to form uniform gran ules. After cooling, these are separated from the water and dried, for example,'inan oven or in a shelf dryer.

EXAMPLE 2 Water-wet cellulose lower alkyl ether iscsuspended in hot water and finely ground wax is slowly added during agitation. The wax melts as it is added to the hot water and in this form is absorbed by the cellulose ether with the formation of a uniform cellulose ether-wax mixture.

After the addition of the desired amount of wax,

enough" to cause swelling.- dry'ethyl cellulose may be stirred or beaten into a ZO'per' cent solution of eth'an'olin waterimethod de scribed in Example *1, wherein I an emulsion of a celluloseether solution is poured'intohot water'- wax suspension, forms a water-wet dispersion of the cellulose ether in which the- 'waxis absorbed. If the cellulose ether'employed in the slui'ly i not water-wet and absorptive, the cellulose ether wax granules are less uniform than those prepared according to thepre'ferred embodiment of the invention.

The actual size and uniformity of the wax-cellulose ether granulesmay vary considerably, but this variation may be controlled by controlling the temperature of granule formation and the agitator speed in the mixing fvess'el; The higher the temperature emp1oyed,the smaller are the granules obtained under otherwise similar condltionsr Likewise with other conditions constant, the higher the agitatorspeed, the smaller the granules produced. V

The proportion of wax to cellulose ether in my product maybe from 2 to per cent of wax for each 98 to io per centof cellulose ether. with these proportions of ingredients, the aforesaid process in either of its 1 described modifications gives a free-flowing granuiarjarticle.

'Themethod may be used to produce useful I granulararticles from any wax in combination with a lower alkyl ether of cellulose, thus montanwax, paramn wax, candelilla wax, hydro- -genated castor oil wax, carnauba wax, Chinese insect wax,-iesparto grass wax ,c.Japan wax, or mixtures of two or more of these substances may be used. The use of hydrogenated castor oil wax in the form of cellulose ether-wax granules is particularly advantageous, since the two components are not soluble in the same volatile solvents, and hence cannot be mixed by forming a common solution of useful concentration.

Of the available organo-soluble cellulose lower alkyl ethers, we prefer to use ethyl cellulose, but we may utilize water-insoluble methyl cellulose,

propyl cellulose, butyl cellulose, or mixed ethers, such as methyl ethyl cellulose, ethyl propyl cellulose, and the like. .The invention is particularly useful and'has particular application in the preparation of a granular article suitable for use in formulating hot-melt coating compositions. These are customarily made by melting together resins, -pl sticizers, and waxes, and dissolving a cellulose e her in the molten mixture. A high temperature is necessary to get a homogeneous melt and the rate of solution of the cellulose ether in the melt is frequently slow. During solution, partial decomposition of the cellulose ether \occurs with concomitant darkening and coloring of the melt. The new granular Products have a lower softening point than that of the cellulose ether which they contain. They melt and disperse in plasticizer-resin mixtures at comparatively low temperatures and in a short period of time, thus reducing the amount of discoloration when forming resin-wax-cellulose ether melts.

The following table illustrates a few of the properties of several ethyl cellulose-wax mix- I claim: l. The method of preparing a uniform gra'n'u lar composition consisting essentially of a cellulose ether and wax, which comprises mixing with agitation a molten wax with an aqueous suspension of a water-wet precipitated cellulose lower alkyl ether at a temperature above the melting point of the wax, cooling to a temperature below the melting point of the wax, and separating -10 the granular particles thereby obtained.

2. The method of preparing a uniform granular composition consisting essentially of ethyl cellulose and wax, which comprises mixing with agitation a molten wax with an aqueous suspen- 15 sion oil water-wet precipitated ethyl cellulose at a temperature above the melting point of the wax, cooling to a temperature below the melting point of the wax, and separating the granular particles thereby obtained.

20 3. The method of preparing a uniform granular composition consisting essentially of ethyl cellulose and hydrogenated castor oil wax which comprises mixing with agitation a molten hydrogenated castor oil wax with an aqueous suspentures in granular form Prepared according to the 2 sion of water-wet precipitated ethyl cellulose at a invention. The ethyl cellulose employedcontains 48.4 per cent ethoxyl and its 5 per cent solution in 80:20 toluene-ethanol has a viscosity of 10 centipoises. A 10 per cent solution in the same solvent has a viscosity of 70 centipoises. The granules were prepared by mixing the required amounts of ethylcellulose and wax according tothe aforesaid process. Uniform granules were formed which were separated from most of the water by centrifuging and dried in a stream of warm air. Viscosity data in the table are expressed ln centipoises and are determined in a 10 per cent solutionkin 80:20 toluene ethanol.

temperature above the melting point of the wax, cooling to a temperature below the melting point of the wax and separating the granular particles thereby obtained.

30 4. The method of preparing a uniform granu- 3 5 ethyl cellulose at a temperature above the melting point of the wax, cooling to a temperature below the melting point of the wax and separating the granular particles thereby obtained.

TABLE I Properties of granular ethyl cellulose compositions comprzsmg war Composition Ethoxy content of composition Softenvw Wax 1 a cosity Ethyl Experi- Theop cellulose mental retical Name Amount Per ,cent Per cent 98 Hydrogenated oastor oil 2 47. 7 47. 95 .do 5 46. 1 46. 0 90 10 43.7 44.0 85 41.2 41.8 70 33.8 33.8 50 50 24.9 24.2 60 21.2 19.6 90 10 44.2 44.0 60 24.6 24.2 90 10 44.5 44.0 50 5O 26. 1 24. 2 90 10 43.6 44.0 50 24.0 24.2 10 43.8 44.0 60 40 28. l 28. 4 0 48.4

It is seen that the experimental and theoretical values for ethoxyl content in the granules agree closely and hence that each batch of granules is quite uniform in composition.

EARLE L. KROPSCOT'I. 

